In this laboratory study, the initial phase of a single-stage sodium bisulfite cook was observed and analyzed. The experiments were carried out using either a lab- or a mill-prepared cooking acid, and the cooking temperature used in these experiments was 154 °C. Investigated parameters were the chemical consumption, the pH profile, and the pulp yield with respect to cellulose, lignin, glucomannan, xylan, and finally extractives. Cooking was extended down to approximately 60% pulp yield and the pulp composition during the cook, with respect to carbohydrates and lignin, was summarized in a kinetic model. The mill-prepared cooking acid had a higher COD (Chemical Oxygen Demand) and TOC (Total Organic Carbon) content than the lab-prepared cooking acid and this influenced the pH and the formation of thiosulfate during the cook. It was found that the presence of dissolved carbohydrates and lignin in the bisulfite cooking liquor affected the extractives removal and the thiosulfate formation.